SU499259A1 - The selection method diacetone - sorbose - Google Patents

Description

(54) METHOD FOR DIACETONE-SULPHOSIS EXTRACT

by bleeding the resulting aqueous and organic layers.

The organic layer containing water, acetone, mesityl oxide and diacetone-b-sorbose is subjected to distillation with hot water (pressure 2 am) or by pre-dilution of the organic layer with water, followed by distillation to isolate the fraction containing water, mesityl oxide, acetone , and fractions (VAT residue) containing 20-25% aqueous solution, i.e. target product (diacetone-b-sorbose). An aqueous layer containing water, sodium sulfate, sodium hydroxide, mono acetone adsorphosis, tar products and traces of acetone, is cooled to - ~ -5-0 ° C to allow anhydrous sodium sulfate. The mother liquor from the crystallizer is mixed with an alkali solution to a concentration of 18-28 wt. % and return to the stage of neutralization.

In the process of isolating diacetum-b-sorbose, but according to the proposed method, all processes are carried out continuously and the duration of the production cycle is reduced to 1 hour. In addition, anhydrous sodium sulfate is separated from the mother liquor, the product is not caking and can be used in the glass industry.

Table 1

T a b .1 and c and 2

Example 1. The neutralization process is carried out in a hollow counter-flow column. The height of the column 3 m, diameter 100 mm. The temperature supplied to the neutralization of the acidic reaction mass is 20 ° C, the temperature at the bottom of the column is 33 ° C, the temperature at the top of the column is 25 ° C. The material balance of the neutralization process is presented in table. one.

The rectification process is carried out in a distant distillation column with perforated plates with an efficiency of 10 theoretical plates. The temperature of the top of the column and the feed mixture is 60 ° C, the temperature of the cube is 100 ° C. Sharp water vapor is supplied to the bottom of the column. The material balance of the rectification process is presented in table. 2

Claims (2)

Invention Formula A method for isolating diacetone-L-sorbose by neutralizing the acidic reaction mass obtained during the synthesis from sorbose and acetone with an aqueous alkaline solution, separating acetone and mesityl oxide, characterized in that, in order to simplify the crystallization process, it is carried out in a screw crystallizer. The temperature in the K | installer + 5 ° C. During crystallization, anhydrous sodium sulfate is released from the mother liquor. Example 2. The stages of the processes preceding the rectification are similar to those shown in Example 1. The rectification process is carried out in a distant distillation column with a set of symmets, and with tracks and an efficiency of 10 theoretical plates. The initial mixture is pre-diluted with the required amount of water over the mat (rial balance shown in Table 3). The temperature of the top of the column and the feed mixture is 60-64 ° C, the temperature of the cube is 100 ° C. Table 3 The process, neutralization is carried out with an 18-28% alkali solution by countercurrently feeding the reaction mass at a ratio of the reaction mass and alkaline solution of 1: 3-6, followed by separation into an aqueous and organic layer, which is rectified with the release of the target product.